1、Tihis standard incorporates the English v.efiuiot f- 6352. F-mnon EeSt I rn Mung dies Ni g rav met ristrh es Veffahreni mit Dirnethplglycmirn (IC0 6552 : 1986) Watiarrral famad This ct-and ard has beem puibii sked i niaccrordan ce- 4% a dhcisi an taken t by CEN/W toadopt,. outialtwafbion, Ihtefnatim
2、nal Standard IS 63% as ai Euriopoarr Stardard. The respcrnsible- Germant body inworlved in1 the- przparatiom Crf-thiis standard was the N4rme;ausschuB Nichtmaenmerrrssln,mrng tio the- intm-diornat Standards, referred tu in1 CIautSL Z af the ENI ase as follbwf: IS0 3s-1 IS0 6481 DIN 12 6913 IC0 1 CL4
3、2 ISQ 5725 IDIN ICQ 5725 DIN 12 7UO Part 1 DIN 12 GE4 Part 1 bandhrds tiefared ta (and not inlcluded in Refererncac) DIMi 12 6641 Pant: 1 Labamtory glasswarel its ownilarrguiiagparrd niotifld to the Gentml Secretariati has the same statusas theofficiaJi uerw o nis. CLEW members m the rraIlIonal stan
4、dard-; bodies of4 FEustriia, EEeel determinatiani af nick dimetylgllocime-gfimetri method wassubmitted to the GEN PQ pmcedsire. Foliohnr.in-g the pcrsitiwe reauilf of tRs RQ! GEM/BT agreed ta Submit IFXI 6352 : 1 %5, w.ithaut modificatiotm, tm AormallVots. This Eumpem Staadardjwas appnoued by GEN om
5、 1991 -11-ojs. In zcmrdhn-cewith thE CEN/CENELEII; Internai Rbgulatiwm, the fallhwingcauntnes are bauind toimplmnt this European1 Standbrd : ndlctz Thetwxtlof Iriterfiational Stmdasd ISQ16352: 188S was approved by GEN asa EuoopiraniCtmndard without any nadifimtiiion. 4.2 ffikrJz acidb usedi t Cnandi
6、ticpo a new CTUEM ar to? clean? a NQTE - For ferrcsnickelsarnpks cantairring me tkn 11 % (m/nr) , use a pel;kteraflworuethyl add, at the end of- effetvesceabiiizy. of 99!9 %. Y The rrm.ri reand r, except far the yb case of ttia EE2 sample. lit is raional trrregad this valusas zero. Stmdardi dwia9on
7、- withini analyst; pWli - ktween analJrSt4twthin labmatury, w2 - ktweetrlabmeries, gb Repeeidability; r = 233 Repmdbcibility; between1 laboratories, R 0,13 o: 19 UDC 669.1524-198 : 620.1 : 543.7 : 546.74 DEUTSCHE NORM February 1992 Determination of nickel content of ferronickel Gravimetric method us
8、ing dimethylglyoxime (IS0 6352 : 1985) English version of DIN EN 26 352 DIN 7 EN 26 352 This standard incorporates the English version of Is0 6352 Ferronickel; Bestimmung des Nickelgehaltes; gravimetrisches Verfahren mit Dimethylglyoxim (IS0 6352 : 1985) European Standard EN 26 352 : 1991 has the st
9、atus of a DIN Standard. A comma is used as the decimal marker. National foreword This standard has been published in accordance with adecision taken byCEN/BTto adopt, without alteration, International Standard IS0 6352 as a European Standard. The responsible German body involved in the preparation o
10、f this standard was the Normenausschu Nichteisenmetalle (Nonferrous Metals Standards Committee). The DIN Standards corresponding to the International Standards referred to in clause 2 of the EN are as follows: IS0 Standard DIN Standard IS0 385-1 IS0 648 DIN 12 690 IS0 1042 IS0 5725 DIN IS0 5725 DIN
11、12 700 Part 1 DIN 12 664 Part 1 Standards referred to (and not included in References) DIN 12 664 Part 1 Laboratory glassware: one-mark volumetric flask with flanged rim, conical socket and conical joint DIN 12 690 Laboratory glassware; classes A and B one-mark bulb pipettes DIN 12 700 Part 1 Labora
12、tory glassware; burettes; general requirements International Patent Classification G O1 N 33/20 EN comprises 8 pages. Beuth Verkg GmbH, Berlin, has the exclusive right of sale for German Standards (DIN-Normen). DIN EN 26352 Engl. Price group 8 06.93 Sales No. 11 08 EUROPEAN STANDARD NORME EUROPENNE
13、EUROPAISCHE NORM EN 26352 November 1991 UDC 669.1524-198 : 620.1 : 543.7 : 546.74 Descriptors: Ferroalloys, ferronickel, chemical analysis, determination of nickel content, gravimetric analysis, dime- thylg lyoxi me. English version Ferronickel Dimethylglyoxime gravimetric method (IS0 6352 : 1985) D
14、etermination of nickel content Ferro-nickel; dosage du nickel; mthode gravimtrique la dimthylglyoxime (IS0 6352 : 1985) Ferronickel; Bestimmung des Nickelge- haltes; gravimetrisches Verfahren mit Di- methylglyoxim (IS0 6352 : 1985) This European Standard was approved by CEN on 1991-11-06 and is iden
15、tical to the IS0 Standard as referred to. CEN members are bound to comply with the CENKENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning suc
16、h national standards may be obtained on application to the Central Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language
17、and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and Unite
18、d Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Centrai Secretariat: rue de Stassart 36, B-1050 Brussels O 1991. Copyright reserved to all CEN members. Ref. No. EN 26 352 : 1991 E Page 2 EN 26 352 : 1991 Foreword In 1991, IS0 6352 :
19、 1985 Ferronickel; determination of nickel content; dimethylglyoxime gravimetric method was submitted to the CEN PQ procedure. Following the positive result of the PQ, CEN/BT agreed to submit IS0 6352 : 1985, without modifications, to Formal Vote. This European Standard was approved by GEN on 1991-1
20、1-06. In accordance with the CENKENELEC Internal Regulations, the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United
21、Kingdom. Endorsement notice The text of International Standard IS0 6352 : 1985 was approved by CEN as a European Standard without any modification. Page 3 EN 26 352 : 1991 1 Scope and field of application This International Standard specifies a gravimetric method for the determination of the nickel
22、content of ferronickel in the range 15 to 60 % (m/rnl. 2 References IS0 385/1, Laboratory glassware - Burettes - Part Ir General requirements. IS0 618, Laboratory glassware - One-mrk pipettes. IS0 1042. laboratory glassware - One-mar voiumtnc ffasks. IS0 5725, Precision of test methods - Determinati
23、on of repeatability and reproduci m, is the mass, in grams, of the empty crucible; m2 is the mass, in grams, of the crucible and the nickel dimethylglyoxime precipitate; Y is the volume, in millilitres, of the aliquot part of the test solution taken in 7.5.1 ; wf (%) is the correction for percentage
24、 of nickel which is determined in the combined filtrates (7.5.11); 203 is the conversion factor, multiplied by 100. of nickel dimethylgfyoxime to nickel. 8.2 Precision 8.2.1 Laboratory tests 8.2.1.1 This International Standard was subjected to an inter- laboratory test programme involving seven coun
25、tries, 20 lab- oratories and 39 analysts. Eight samples of commercial ferro- nickel covering the range of 21 to 41 % (mlm) nickel were analysed. Each laboratory was requested to supply two deter- minations by each of WO analysts for each sample. 8.2.1.2 The test was carried out on test solutions of
26、50 ml for nickel contents lower than 30 % (mim) and 25 ml for contents higher than 30 % (m/m). These solutions became 100 ml and 50 ml, respectively, in the final procedure adopted after com- pletion of the programme (see 7.5.1). It ic expected that the repeatability and the reproducibility will be
27、better when the method is used as specified. 8.2.2 Statistical results Repeatability and two reproducibilities were calculated accord- ing to the principles of IS0 5725. The values resulting from this analysis are given in table 1. A report on the interlaboratory tests and statistical analysis is gi
28、ven in annex B. Table 1 - Results of statistical analysis Nickel content %rn/m)l Standard deviation - within analyst, .y, - between analydwithin laboratory, .sw2 - between laboratories, .sb Repeatability, r = 2.83 e, Reproducibility, within laboratory, R, R, = 2.83 4m2 Reproducibility. between labor
29、atories, R R = 2.83 15 to 30 0,047 0,047 0,054 0,13 0.19 0.24 31 to45 0.066 0,095 0,047 0.19 0,s 0.35 NOTES TO TABLE 1 1 These values of the repeatability and reproducibility can be retained as normally representative of the performance of the analytical method specified in this International Standa
30、rd and applied to similar samples. 2 The repeatability and reproducibility data may be used as guidelines for establishing splitting limits. 9 Test report The test report shall include the following information : a) the reference to the method used: bl the results of the analysis; c) the number of i
31、ndependent replications; d any unusual features noted during the analysis: e) any operation not included in this International Stan- dard or regarded as optional. Page 6 EN 26 352 : 1991 Annex A Determination of nickel in combined filtrates by atomic absorption spectrometry (This annex forms an inte
32、gral part of the Standard.) A.l General This annex describes the procedure for the determination of residual nickel in the combined filtrates from the gravimetric determination of nickel (see 7.5.10 and 7.5.11). A.2 Reagents A.2.1 Hydrochloric acid, 0, = 1,19 g/ml. A.2.2 Ni per litre. Weigh, to the
33、nearest 0,005 g, 1,00 g of nickel metal, 99,9 % (mlm minimum, transfer to a 600 ml beaker and dissolve in 40 ml nitric acid (orn = 1.41 g/ml) diluted 1 +1. Evaporate to a viscous syrup, cool, redissolve the salts in water and transfer to a 1 O00 mi one-mark volumetric flask. Make up to the mark with
34、 water and mix. Nickel, standard solution, corresponding to 0,l g of Pipette 25,0 ml of this solution into a 250 ml one-mark volumetric flask. Make up to the mark with water and mix. 1 ml of this standard solution contains 0,l mg of Ni. A.3 Apparatus Ordinary laboratory apparatus, and A.3.1 O,5 ml,
35、in accordance with IS0 Sil, class A. Burette, of capacity 50 ml, graduated in divisions of A.3.2 Volumetric flasks, of capacities 200; 250: and 1 o00 ml, in accordance with tS0 1042, class A. A.3.3 Pipette, of capacity 25 ml, in accordance with IS0 648, class A. A.3.4 Atomic absorption spectrometer,
36、 equipped with a burner head for an air-acetylene flame and a nickel hollow cathode lamp. A.4 Procedure A.4.1 Adjustment of atomic absorption spectrometer Set the required instrument parameters according to the manufacturers instructions. Adjust the wavelength to 232 nm and the nickel lamp current a
37、s recommended. Light the burner and adjust the flows of air and acetylene to ob- tain an oxidizing, clear, non-luminescent flame while aspirating water. Adjust the instrument to zero. A.4.2. Preparation of the set of calibration solutions Transfer, using a burette, O; 2; 5; 10; and 15 ml of the nick
38、el standard solution (A.2.2) to each of five 200 ml one-mark volumetric flasks. Add 50 ml of hydrochloric acid (A.2.11, make up to the mark with water and mix. These calibration solutions correspond to 0,O; 0,2; 0,5: 1,O; and 7,5 rng of Ni in the200 ml volume (see 7.5.10). A.4.3 Atomic absorption me
39、asurements Aspirate each of the calibration solutions A.4.2) starting with the zero member and note the absorbance reading. Flush the system by aspirating water between each reading. Aspirate the test solution (7.5.10) and note the absorbance reading. Repeat the measurement of calibration solutions
40、and test sol- ution such that the measurement of the test solution lies be- tween the measurement of two calibration solutions. A.4.4 Preparation of the calibration graph Plot the instrument reading against the nickel content of the calibration solutions. A.5 Expression of results Using the calibrat
41、ion curve (A.4.4) read the amount of nickel corresponding to the measured absorbance of the test solution. The nickel content of the filtrates, wf (%I, to be applied as a cor- rection in 8.1, expressed as a percentage by mass of the original sample, is given by the formula m3 x 100 mg x V where mo i
42、s the mass, in grams, of the test portion (7.11: m3 is the mass, in milligrams, of nickel in the test solution: V is the volume, in millilitres, of the aliquot of the test solution taken in 7.5.1. NOTES 1 For some atomic absorption instruments it may be necessary to use scale expansion. 2 It is not
43、necessary to add dimethylglyoxime to the calibration sol- utions and evaporate to a viscous consistency for mineralization. 3 If the nickel content of the test solution is high then it may be diluted by a known amount and an appropriate correction made. Page 7 EN 26 352 : 1991 Annex B Statistical re
44、port of interlaboratory tests (This annex is given for information only.) B.O Introduction This International Standard was tested in an interlaboratory programme involving seven countries, 20 laboratories and 39 analysts. Eight samples of commercial ferronickel covering the range 21 to 41 % (rn/m) w
45、ere analysed for nicket content. The test programme was designed to determine the repeatability and the within- and between-laboratory reproducibilities in general, in the same spirit as IS0 5725. B.l References IS0 3534, Statistics - Vocabulary and symbols. IS0 5725, Precision of test methods - Det
46、ermination of repeatability and reproducibility by inter-laboratory tests. B.2 Definitions For the purpose of this annex, the definitions of IS0 3534 apply. Complementary information was added in the within-laboratory reproducibility which was represented by the factor of a change in analyst within
47、a laboratory. B.3 Design of test programme The analytical test programme was designed with the aim of providing maximum information. Each laboratory was re- quested to analyse each sample in duplicate by two analysts. Thus for each participating laboratory, two pairs of results for each sample are o
48、btained. 6.4 Test samples This test programme used eight samples of ferronickel in the form of chips obtained by milling or drilling of ingots; in the case of milling, the chips were crushed in a vibratory crusher. These samples had nickel contents ranging from 21 to 41 96 (m/m) and represented comm
49、ercial qualities. 8.5 Changes in analytical procedure The test was carried out by taking aliquots of 50 ml for contents lower than 30 % h/m) in nickel and 25 ml for contents higher than 30 % (rn/rn). These aliquots have become 100 ml and 50 ml, respectively, in the final procedure adopted after com- pletion of the test programme (see 7.5.1 ). B.6 Statistical procedures B.6.1 Statistical tests for outliers B.6.1.1 As recommended in IS0 5725, Cochrans test was applied to compare the within-analyst fluctuations (variance of repeatability o
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